CN1957650B - Electromagnetic wave shielding material and process for producing the same - Google Patents
Electromagnetic wave shielding material and process for producing the same Download PDFInfo
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- CN1957650B CN1957650B CN200580016522XA CN200580016522A CN1957650B CN 1957650 B CN1957650 B CN 1957650B CN 200580016522X A CN200580016522X A CN 200580016522XA CN 200580016522 A CN200580016522 A CN 200580016522A CN 1957650 B CN1957650 B CN 1957650B
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0094—Shielding materials being light-transmitting, e.g. transparent, translucent
- H05K9/0096—Shielding materials being light-transmitting, e.g. transparent, translucent for television displays, e.g. plasma display panel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
- H01J2211/20—Constructional details
- H01J2211/34—Vessels, containers or parts thereof, e.g. substrates
- H01J2211/44—Optical arrangements or shielding arrangements, e.g. filters or lenses
- H01J2211/446—Electromagnetic shielding means; Antistatic means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
- Y10T428/2809—Web or sheet containing structurally defined element or component and having an adhesive outermost layer including irradiated or wave energy treated component
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Abstract
An electromagnetic wave shielding material that exhibits a high electromagnetic wave shielding effect, excelling in transparency and sight through property; and a process for producing the electromagnetic wave shielding material simply and easily at low cost. There is provided a process for producing an electromagnetic wave shielding material, characterized by first providing a transparent resin base material having a transparent porous layer composed mainly of at least one member selected from the group consisting of oxide ceramics, nonoxide ceramics and metals; subsequently screen printing the surface of the transparent porous layer with a conductive paste containing granular silver oxide, a silver salt of tertiary fatty acid and a solvent into geometrical pattern; and thereafter heating so that a conductive part of geometrical pattern is disposed on the surface of the transparent porous layer. Further, there is provided an electromagnetic wave shielding material produced by this process.
Description
Technical field
The electromagnetic shielding material that the present invention relates to be used for the electromagnetic shielding that will take place from electric equipments such as CRT, PDP with and manufacture method.
Background technology
All the time, on base material, form pattern, make the article of the various character of utilizing its electric character, magnetic etc. with conductivity or magnetic.Wherein, in order to cover the electromagnetic wave that leaks from the front face side of display parts such as CRT, PDP, the electromagnetic wave shielding plate is provided at the front of display screen, is widely used as front panel.As the electromagnetic wave shielding plate that front panel uses, except the function of electromagnetic wave shielding, also requirement does not reduce the perspectivity of the display frame of display screen.
As the electromagnetic shielding material that possesses perspectivity and electromagnetic wave shielding performance two aspects, following report example is arranged: for example use electroconductive powder and adhesive, by on transparent resin base material surface, carrying out the electromagnetic shielding material with conductive part (patent documentation 1 and 2) that silk screen printing forms.
But, utilize silk screen printing usually, forming with the clathrate pattern under the situation of screen, the printing that the broken string of moire, fine rule or line chap etc. take place easily because of the interference with the gauze eye of printed panel is bad, is not easy to carry out the printing of precision.Therefore, the problem that the electromagnetic wave shielding performance is low or perspectivity is low takes place easily.
Patent documentation 1: the spy opens flat 11-26984 communique
Patent documentation 2: the spy opens the 2001-196784 communique
Summary of the invention
The object of the present invention is to provide the electromagnetic shielding material of electromagnetic shielding effect height, the transparency and perspectivity excellence, and the easy and cheap manufacture method of this electromagnetic shielding material.
The present inventor has carried out intent research in order to address the above problem, found that: be selected from oxide ceramics possessing to contain, on at least a kind of this transparent porous aspect in non-oxide ceramics and the metal as the transparent resin base material of the transparent porous layer of principal component, with the geometry pattern specific conductive paste is carried out after the silk screen printing, by under lower temperature, calcining, on this transparent porous aspect, can form the conductive part of the geometry pattern of the broken string that almost do not have fine rule and line chap, can produce and have excellent electromagnetic wave shielding performance, the electromagnetic shielding material of the high aperture (perspectivity) and the transparency.On the basis of this understanding, finished the present invention through further discussing repeatedly.
That is, the invention provides following electromagnetic shielding material with and manufacture method.
(1) a kind of manufacture method of electromagnetic shielding material, it is characterized in that, contain at least a kind of this transparent porous aspect that is selected from oxide ceramics, non-oxide ceramics and the metal possessing as the transparent resin base material of the transparent porous layer of principal component, the conductive paste that will contain particle shape silver oxide, uncle's aliphatic acid silver and solvent carries out after the silk screen printing with the geometry pattern, with the transparent resin base material heat treated of this printing, on this transparent porous aspect, form the conductive part of geometry pattern.
(2) manufacture method of being put down in writing according to (1) is characterized in that aforementioned transparent resin base material has hard conating on the face opposite with transparent porous layer.
(3) manufacture method of being put down in writing according to (1) or (2), it is characterized in that it directly is that 2 μ m or lower particle shape silver oxide, total carbon atom number are the silver salt of uncle's aliphatic acid of 5～30 and will be selected from the ether-ether class of aromatic hydrocarbon, ethylene glycol, the ether-ether class of propylene glycol and at least a kind of solvent as principal component in the terpineol that aforementioned conductive paste contains averaged particles.
(4) according to any manufacture method of being put down in writing in (1)～(3), it is characterized in that aforementioned transparent porous layer thickness is about 0.05～20 μ m.
(5) according to any manufacture method of being put down in writing in (1)～(4), it is characterized in that, aforementioned transparent porous layer contains at least a kind of atomic aggregate as principal component that will be selected from silica, titanium oxide and the aluminium oxide, and has pore between this particulate.
(6) manufacture method of being put down in writing according to (5) is characterized in that the averaged particles of aforementioned micro particles directly is about 10～100nm, and aforementioned fine pore is about 10～100nm.
(7) manufacture method of being put down in writing according to (1), it is characterized in that aforementioned transparent porous layer is to form by being selected from a kind of method that intaglio plate coating, hectograph coating, comma coating (comma coating), mouthful mould coating (die coating), slit coating, spray-painting, plating be coated with in method, sol-gel process, LB embrane method, CVD, evaporation, sputter, the ion plating.
(8) manufacture method of any electromagnetic shielding material of being put down in writing of basis (1)～(7) is characterized in that the temperature of aforementioned heat treated is about 150～200 ℃.
(9) any manufacture method of being put down in writing of basis (1)～(8), it is characterized in that the resin of aforementioned transparent resin base material is at least a kind that is selected from mylar, polycarbonate resin, poly-(methyl) acrylate, silicone resin, cyclic polyolefin resin, polyarylate resin and the polyethersulfone resin.
(10) according to any manufacture method of being put down in writing of (1)～(9), it is characterized in that aforementioned transparent resin base material is sheet, membranaceous or tabular.
(11) a kind of electromagnetic shielding material is characterized in that, it is to make by any manufacture method of being put down in writing of (1)～(10).
(12) electromagnetic shielding material of being put down in writing according to (11) is characterized in that the live width of the geometry pattern of conductive part is about 10～30 μ m, and aperture opening ratio is about 80～95%.
(13) a kind of membranaceous electromagnetic shielding material, it is the electromagnetic shielding material that has the conductive part of geometry pattern on transparent resin base material, it is characterized in that, full light transmittance is 72～91%, turbidity value is 0.5～6%, sheet resistance value is 5 Ω/ or littler, and the geometry pattern line-width of conductive part is about 10～30 μ m, and aperture opening ratio is about 80～95%.
(14) electromagnetic shielding filter used of a kind of plasma display panel (PDP) is characterized in that, contain (11)～(13) in any electromagnetic shielding material of being put down in writing.
(15) method of the conductive part of formation geometry pattern on transparent porous aspect, it is characterized in that, contain at least a kind of this transparent porous aspect that is selected from oxide ceramics, non-oxide ceramics and the metal possessing as the transparent resin base material of the transparent porous layer of principal component, the conductive paste that will contain particle shape silver oxide, uncle's aliphatic acid silver and solvent with the geometry pattern carries out carrying out heat treated after the silk screen printing.
Below, describe the present invention.
The manufacture method of electromagnetic shielding material of the present invention, it is characterized in that, contain at least a kind of this transparent porous aspect that is selected from oxide ceramics, non-oxide ceramics and the metal possessing as the transparent resin base material of the transparent porous layer of principal component, the conductive paste that will contain particle shape silver oxide, uncle's aliphatic acid silver and solvent with the geometry pattern carries out after the silk screen printing, base material after further will printing carries out heat treated (calcining), forms the conductive part of geometry pattern on this transparent porous aspect.
Transparency resin base material
As the substrate resin of the transparent resin base material that uses in the present invention, be thermal endurance height and transparent, as long as can form the material of this transparent porous layer on this base material, just there is no particular limitation.
The mylar, polycarbonate resin, poly-(methyl) acrylate, silicone resin, cyclic polyolefin resin, polyarylate resin, polyethersulfone resin of PETG (PET), PEN (PEN) etc. etc. particularly, can example be shown.Wherein, comprehensively judge, preferably adopt mylar, especially preferably adopt PET or PEN from the viewpoint of the transparency, cost, durability, thermal endurance etc.
At this, the transparency on transparent resin base material, so long as can be used in the transparency of purposes degree of the display part of PDP, CRT etc., just there is no particular limitation.Usually, the full light transmittance of measuring according to JISK7105 is about 85～90%, and the turbidity value of measuring according to JIS K7105 is about 0.1～3%.
The form of transparency resin base material can be used in the form of the display part of PDP, CRT etc.,, adopts membranaceous, sheet, tabular etc. that is.This form can be by known method with above-mentioned substrate resin manufacturing.
On transparent resin base material of the present invention, have and contain at least a kind of the transparent porous layer that is selected from oxide ceramics, non-oxide ceramics and the metal as principal component.
At this, can the simple oxide of titanium oxide, aluminium oxide, magnesium oxide, berylia refractories, zirconia, silica etc., the composite oxides of the silicate of silica, forsterite, talcum, wollastonite, zircon, mullite, cordierite, spodumene etc., aluminium titanates, spinelle, apatite, barium titanate, PZT, PLZT, ferrite, lithium niobate etc. be shown example as oxide ceramics.
The carbon that the carbide, amorphous carbon, graphite, diamond, case crystalline sapphire etc. of the nitride, carborundum, boron carbide, titanium carbide, tungsten carbide etc. of silicon nitride, silicon aluminum oxygen nitrogen heat-stable ceramic (Sialon), aluminium nitride, boron nitride, titanium nitride etc. can example be shown as non-oxide ceramics.In addition, can boride be shown example. sulfide. silicide.
As metal, can gold, silver, iron, copper, nickel etc. be shown example.
Can use in them at least a kind as raw material, more preferably silica, titanium oxide, aluminium oxide, other composition or cooperate that there is no particular limitation.
On transparent resin base material, form the method for transparent porous layer, can be the wet processing process, also can be the dry process process, have no particular limits, but consider preferred wet processing process from the angle of productivity and cost.The wet processing process can be by known method coating (coating) on base material.As the method for coating, intaglio plate coating, hectograph coating, comma coating, mouthful mould coating, slit coating, spray-painting, plating for example can example be shown be coated with method, sol-gel process, LB embrane method etc., special preferred sols-gel method.As the initiation material of sol-gel process, for example, can enumerate tetraethoxysilane, methyl triethoxysilane, tetrachloro silicane, the tri sec-butoxy aluminum when aluminium oxide, 2 when silica, the 4-pentanedione closes aluminium (III) etc.In the presence of catalyst, water, make above-mentioned initiation material carry out sol gel reaction, also can will carry out their hydrolysate (reaction intermediate) of sol gel reaction as initiation material.In addition, as required, also can suitably add other compositions of resin, surfactant etc.As the dry process process, for example, can CVD, evaporation, sputter, ion plating etc. be shown example.
The transparent porous layer thickness that has on the transparent resin base material that the present invention uses is about 0.05～20 μ m, particularly about 0.1～5 μ m.
In addition, this transparent porous layer contains at least a kind of atomic aggregate (agglutination body) as principal component that will be selected from oxide ceramics, non-oxide ceramics and the metal, has pore between particulate.The averaged particles of this transparent porous layer directly is about 10～100nm, and this fine pore is about 10～100nm.In the present invention owing to have a such a transparent porous layer, so with the coupling excellence of conductive paste described later, can form the pattern of hope.
Form with transparent resin base material of transparent porous layer is, membranaceous, sheet, tabular etc.Under the situation of membranaceous or sheet, the thickness with transparent resin base material of transparent porous layer is generally about 25～200 μ m, is preferably about 40～188 μ m.Particularly under situation about using, be preferably about 50～125 μ m as the comprehensive electromagnetic shielding material of the display screen of PDP etc.In addition, under tabular situation, its thickness is generally about 0.5～5mm, can be preferably about 1～3mm.
The transparency with transparent resin base material of transparent porous layer, usually, the full light transmittance of measuring according to JIS K7105 is about 85～90%, and the turbidity value of measuring according to JIS K7105 is about 0.1～3%.
Also have, on the transparent resin base material of Shi Yonging, on the face opposite, hard conating can be set in the present invention with above-mentioned transparent porous layer.
As hard conating,, have no particular limits so long as, just can use general material without detriment to the material of the transparency.Wherein preferred UV cured type acrylic resin.As its principal component, just there is no particular limitation so long as polyester acrylate, urethane acrylate, epoxy acrylate etc. have the acrylate of 2 or more multi-functional UV cured type.Preferably use as 1, the 6-hexanediyl ester, tripropylene glycol diacrylate, the TEG acrylate, 1,9-nonanediol diacrylate, tristane dimethanol diacrylate, neopentyl glycol PO modification diacrylate, 2 degree of functionality acrylate that EO modified bisphenol A diacrylate is such, or picture trimethylolpropane triacrylate, pentaerythritol triacrylate, two (trimethylolpropane) tetraacrylate, two (pentaerythrites), six acrylate, trimethylolpropane EO modification triacrylate, PO modified glycerol triacrylate, the polyfunctional acrylic ester that trihydroxy ethyl isocyanurate triacrylate is such etc.
In addition, in the acrylate of UV cured type, usually, add Photoepolymerizationinitiater initiater and use.As Photoepolymerizationinitiater initiater,, can be hardened by overlay film fully by adding 1-hydroxycyclohexylphenylketone (IRGACURE 184CHIBASPECIALITYCHEMICALS Co., Ltd. system), 2-hydroxy-2-methyl-1-1-phenyl-propane-1-ketone etc.In addition, also can use the Photoepolymerizationinitiater initiater of benzoin, benzoin derivatives, benzophenone, benzophenone derivates, thioxanthones, thioxanthones, thioxanthone derivates, benzyl dimethyl ketal, alpha-aminoalkyl benzophenone, oxidation monoacyl phosphine, oxidation diacyl phosphine, alkyl (ア Le Network Le) phenyl glyoxylic acid ester, diethoxy acetophenone, two cyclopentadiene titanium compounds etc.
With respect to UV cured type acrylate 100 weight portions, the cooperation ratio of these Photoepolymerizationinitiater initiaters is preferably 1～10 weight portion.When being discontented with 1 weight portion, fully initiated polymerization in addition, when surpassing 10 weight portions, has the situation that durability reduces.
In addition, in aforesaid UV cured type acrylate, under the condition of not damaging its transparent degree, can contain the 3rd composition (UV absorbent, filler etc.), have no particular limits.
On transparent resin base material, form the method for hard conating, can use general coating process, have no particular limits.
By on transparent resin base material, hard conating being set, when calcining described later, can control because oligomer produces albefaction or flavescence from separating out of substrate resin, thus, can guarantee the high transparent of electromagnetic shielding material of the present invention.In addition, can prevent scar in the manufacturing process of electromagnetic shielding material.
Conductive paste
The conductive paste that uses among the present invention is to contain particle shape silver oxide, the material of uncle's aliphatic acid silver and solvent.
The average grain diameter of this particle shape silver oxide is 2 μ m or lower, and when using than directly silver oxide of its bigger particle, in the manufacture process (mixing operation, synthesis procedure etc.) of conductive paste, its average grain diameter can be made as 2 μ m or lower.More preferably average grain diameter is 200～500nm.If using average grain diameter is 2 μ m or lower particle shape silver oxide, then easy mesh by half tone, can suppress to be printed on the broken string of the fine rule on the transparent porous layer or to ooze out, and the thermal decomposition of the reduction of silver oxide and uncle's aliphatic acid silver can be carried out under lower temperature, thereby preferred.
Uncle's fatty acid silver salt is meant that total carbon atom number is 5～30, is preferably the silver salt of uncle's aliphatic acid of 10～30, can dissolve and even be dispersed in the dispersion solvent that uses when making thickener.This uncle's fatty acid silver salt plays the effect of lubricant, in that silver oxide and uncle's fatty acid silver salt are mixing when becoming pasty state, silver oxide is pulverized and are promoted corpusculed, and exist around the silver oxide particle, suppresses the aggegation again of silver oxide particle, makes dispersed the raising.Therefore, can not become pasty state even do not add adhesive yet.In addition, this uncle's fatty acid silver salt has when heating separates out silver, makes from the function of welding between the silver particles of silver oxide reduction generation.
As the object lesson of such uncle's fatty acid silver salt, can enumerate trimethylace tonitric silver, neoheptane acid silver, new nonane acid silver, new decane acid silver etc.The manufacturing of uncle's fatty acid silver salt is undertaken by following, for example, by alkali compounds uncle's aliphatic acid is neutralized in water, makes silver nitrate and its reaction then.
The weight of silver oxide is made as A, when the weight of uncle's fatty acid silver salt is made as B, the particle shape silver oxide in conductive paste and the cooperation ratio of uncle's fatty acid silver salt, preferred weight ratio (A/B) is 1/4～3/1.
In addition, in conductive paste, except silver oxide and uncle's fatty acid silver salt, contain solvent.For this solvent, so long as with silver oxide and uncle's fatty acid silver salt Fails To Respond, just there is no particular limitation to make the material that they disperse well.For example, can use the aromatic hydrocarbon of toluene etc., the ether-ether class of the ethylene glycol of triethylene glycol single-butyl ether etc., the ether-ether class of the propylene glycol of tripropylene glycol n-butyl ether etc., the organic solvent of terpineol etc.With respect to particle shape silver oxide 100 weight portions, the use amount of solvent can be about 1～100 weight portion.
In addition, as required, can add dispersant particle shape silver oxide is disperseed well, prevent the secondary aggegation of particle shape silver oxide.In this dispersant, can use cellulose-based macromolecules such as hydroxy propyl cellulose, PVP, the water soluble polymer of polyvinyl alcohol etc. etc.With respect to particle shape silver oxide 100 weight portions, its use amount can be 0～20 weight portion.
The manufacturing of conductive paste of the present invention can followingly be carried out, and for example, after particle shape silver oxide and uncle's fatty acid silver salt and solvent, carries out with method of mixing one-tenth pasty states such as roller mill etc.This conductive paste is because to have average grain diameter be 2 μ m or lower particle shape silver oxide, so even under the heating condition than lower temperature, also generating behind the metallic mutually at an easy rate, welding becomes filming of continuous argent or piece.
In addition, conductive paste is supplied with silk screen printing after being modulated into the viscosity that is suitable for silk screen printing and thixotropy.Viscosity and thixotropic modulation can suitably be selected according to the kind of the particle of particle shape silver oxide footpath, uncle's fatty acid silver salt, solvent types etc.For example, the viscosity of conductive paste be get final product about 10～10000dPas, the thixotroping index can suitably be chosen as the scope about 0.1～0.9.
For such conductive paste, for example have that Teng Cang changes into society's system, trade name " DOTITEXA-9080 " or " DOTITE XA-9083 " etc.
Electromagnetic shielding material
Electromagnetic shielding material of the present invention, be by with above-mentioned conductive paste after carrying out silk screen printing on the transparent porous aspect of transparent resin base material, heat treated is made.
In the present invention, be feature so that specific conductive paste is carried out silk screen printing on the transparent porous layer of regulation, form the pattern conductive part that does not almost have the broken string of fine rule or ooze out thus.
The method of silk screen printing has no particular limits, and can use known method to carry out.Print employed half tone, can use to have formation shielding electromagnetic wave efficiently, and can guarantee the pattern of the conductive part of sufficient perspectivity degree, particularly have the material of the continuous geometry pattern of clathrate, mesh shape etc.For example, can enumerate on 360～700 purpose stainless steel yarns of stainless steel wire braiding that with diameter are 11～23 μ m, be provided with about live width 10～30 μ m, the half tone of the clathrate pattern about decorative pattern spacing 200～400 μ m.
In silk screen printing of the present invention,, in pattern, take place uneven hardly because of use contains the conductive paste of fine particle shape silver oxide.In addition, because matching of this conductive paste and transparent porous layer on the fine rule of the pattern that forms on the transparent porous layer, takes place to break or ooze out hardly.
In general, by the live width of the pattern of silk screen printing, have in theory than the live width of the half tone tendency of chap a little, but take place hardly line departing from or the distortion of pattern at interval, almost the pattern of the pattern of faithful to half tone is reproduced on the transparent porous layer.Under the situation of the tendency of not wishing to have chap a little, can with the finedraw of half tone wide be set at littler than the live width of desired formation on transparent porous layer, so long as those skilled in the art just can easily carry out this setting.
Then, the electromagnetic shielding material with silk screen printing carries out heat treated (calcining), the conductive part of formation clathrate pattern on transparent porous layer under the low temperature of (particularly about 160～180 ℃) about 150～200 ℃.As mentioned above owing to use specific conductive paste, so even under heating condition than lower temperature, also can take place easily metallic silver corpuscle welding, form filming of continuous argent.In heat treated, for example, can adopt external heat mode (steam or electric heating hot blast, infrared heater, hot-rolling etc.), inner mode of heating (inducing heating, high-frequency heating, resistance heating etc.) etc.Be generally 5 fens heating time～about 120 minutes, preferred about 10 minutes～40 minutes.
Aforementioned heat treated (calcining) can be carried out the multistage.For example, can followingly carry out: as the 1st stage after 50～60 ℃ of heat treated are about 10～20 minutes, and then as the 2nd stage 160～180 ℃ of heat treated about 10～40 minutes.Because the multistage, can be earlier by making solvent evaporates, and then suppress to ooze out.
So, use above-mentioned conductive paste, film the harmful effect that causes so can avoid Yin Re transparent resin base material because can form silver at low temperature and in the short time.That is, can suppress to separate out from transparent resin base material and cause this base material albefaction or cause base material flavescence etc. because of thermal conductance because of thermal conductance causes oligomer.
The albefaction or the flavescence of substrate resin in the time of can further being suppressed at calcining in addition, are arranged under the situation of hard conating at the opposing face with the transparent porous layer of transparent resin base material.
As mentioned above, make electromagnetic shielding material of the present invention.Electromagnetic shielding material of the present invention has high aperture, for example, is 75% or higher, particularly reaches about 80～95%.Thus, can reach high perspectivity.In addition, in this manual, aperture opening ratio is meant in cancellate 1 pattern of the electromagnetic shielding material that Fig. 4 represents, (area B/area A) * 100 (%).
In addition, the live width (W) of the clathrate of conductive part or mesh-shape pattern is generally about 10～30 μ m, about preferred 15～20 μ m.Be approximately the geometry pattern of less than 10 μ m for live width, the tendency of the difficulty made is arranged, if surpass 30 μ m, because pattern has easily attached to the tendency of mesh thereby not preferred.
The interval (spacing) of the clathrate of printing or the line of mesh-shape pattern (P) in the scope that satisfies above-mentioned aperture opening ratio and live width, can suitably be selected.Usually, can be scope about 200～400 μ m.
The thickness of fine rule (in the maximum height of the fine rule of transparent porous aspect vertical direction), though can change according to live width etc.,, be generally about 1 μ m or bigger, particularly about 1～30 μ m.
In addition, the section with the fine rule on the transparent porous layer of silk screen printing formation is the semicircular shape.Report in the past pass through the fine rule that litho method, plating such as are coated with at the pattern that obtains, the section of its fine rule nearly all is rectangular.Therefore, during the adhesive layer of fitting in the above etc., bubble is residual easily, and perspectivity is had harmful effect (Fig. 5 (b)).To this, because the section of fine rule of the present invention is the semicircular shape, tack height, bubble are not easy residual during with applyings such as adhesive layers.The advantage (Fig. 5 (a)) that therefore, the electromagnetic shielding material that can obtain the perspectivity excellence is arranged.
Electromagnetic shielding material of the present invention has high electromagnetic shielding effect, the transparency and perspectivity excellence.And, because the fine rule of conductive part does not almost break, so have the low feature of resistance.The sheet resistance of electromagnetic shielding material of the present invention is 5 Ω/ or lower, is preferably 3 Ω/ or lower, more preferably 2 Ω/ or lower.Sheet resistance value is considered from the angle of shielding character under excessive situation, and is not preferred.
At this,,, can design the sheet resistance value of shielding material with conductive pattern by the live width and the spacing of pattern are set arbitrarily from following formula.
R＝Rs×(P/W)
Rs＝ρv/t
R: sheet resistance value (Ω/) with shielding material of conductive pattern
Rs: the sheet resistance value of conductive paste (Ω cm)
ρ v: the volume intrinsic resistance of conductive paste
T: the thickness of conductive paste
P: the interval (spacing) of clathrate or mesh-shape pattern
W: the live width of clathrate or mesh-shape pattern
The full light transmittance of electromagnetic shielding material of the present invention (JIS K7105) can reach the high value about 72～91%.In addition, turbidity value (JIS K7105) is reduced to about 0.5～6%.
And then the conductive pattern that forms on transparent porous layer is substantially devoid of the additive of adhesive, curing agent, catalyst etc., and its major part contains silver particles basically, and the direct welding of this silver particles is combined into highly purified silver bullion.Therefore, electromagnetic shielding material of the present invention has lower and stable resistance value.
In addition, electromagnetic shielding material of the present invention, on the conductive part that forms on the transparent porous layer, can the stacked guard film.This diaphragm can use normally used known resin.Known method such as stacked with dry method, that wet method is stacked is with these laminated resins.
Electromagnetic shielding material of the present invention, can further stacked functional membrane etc.As functional membrane, can enumerate the antireflection film of the antireflection layer that is provided with the surface light reflection that prevents film, by painted or coloring film, absorption that additive is colored or reflect near infrared near-infrared shielding film, prevent that polluter such as fingerprint is at the anti fouling performance film of surface adhesion etc.
Electromagnetic shielding material of the present invention, electromagnetic shielding effect height, the transparency and perspectivity excellence.In addition, use the manufacture method of silk screen print method of the present invention, can be with the geometry pattern high accuracy of the conductivity of homogeneous, be arranged on the base material easily.Therefore, even be applicable to the electromagnetic wave shielding front panel of the display screen that display area is big, also can make simply.Therefore, except the cathode ray tube (CRT) etc., be useful as the electromagnetic shielding filter that on big display screen such as the display frame of picture plasma display panel (PDP) (PDP) etc., uses.
The manufacture method of electromagnetic shielding material of the present invention, it is characterized in that, with specific conductive paste, on base material, be provided with, contain at least a kind of the transparent porous layer that is selected from oxide ceramics, non-oxide ceramics and the metal as principal component, carry out silk screen printing, can form the broken string that almost do not have fine rule or the conductive pattern of chap thus.
In addition, formed this conductive paste of pattern owing to can so can suppress the albefaction or the flavescence of transparent resin base material, keep the transparency in low temperature calcination.Particularly for the situation of transparent resin base material, when the calcining of this conductive paste, owing to suppressed the influence of heat or moisture by hard conating, so kept the higher transparency to base material with hard conating.Certainly, in the present invention, owing to use silk screen printing, process number is few, easy, and the cost aspect is also favourable, electromagnetic shielding material a large amount of, the quantity-produced productivity is also high.
In addition, electromagnetic shielding material of the present invention with above-mentioned manufacture method manufacturing, because fine rule does not almost break in conductive pattern, can bring into play low, the high electromagnetic shielding effect of resistance value, in addition, because also can suppress the chap of fine rule, so guaranteed the high aperture (perspectivity) and the transparency.
Therefore, be useful especially as the electromagnetic shielding filter that on big display screen such as the display frame of picture cathode ray tube (CRT), plasma display panel (PDP) (PDP) etc., uses.
Description of drawings
[Fig. 1] is the light microscope (multiplying power: observation figure * 100) of graticule of the conductive part of the electromagnetic shielding body that obtains at embodiment 1.
[Fig. 2] is the light microscope (multiplying power: observation figure * 100) of graticule of the conductive part of the electromagnetic shielding body that obtains at comparative example 1.
[Fig. 3] is the light microscope (multiplying power: observation figure * 100) of graticule of the conductive part of the electromagnetic shielding body that obtains at comparative example 2.
[Fig. 4] is the ideograph of the assay method of expression aperture opening ratio.
[Fig. 5] is the profile of the fine rule of expression conductive pattern.
Embodiment
Below, the present invention will be described in more detail according to comparative example and embodiment, but the present invention is not limited to these.
Be determined at the electromagnetic shielding effect that embodiment, comparative example represent in order to following method, full light transmittance, turbidity value, sheet resistor, live width, aperture opening ratio, line is thick.
1. electromagnetic shielding effect
Determinator with Northwest electronics industry development center method (being commonly referred to as the KEC method) is measured.
2. full light transmittance
According to JIS K7105, measure with nephelometer NDH-20D type (Japanese electric look Industrial Co., Ltd system).
3. turbidity value
According to JIS K7105, measure with nephelometer NDH-20D type (Japanese electric look Industrial Co., Ltd system).
4. sheet resistor
Measure with LORESTA EP (DIAINSTRUMENTS corporate system).
5. live width
Use light microscope determining.
6. aperture opening ratio
Use light microscope, measure the live width of cancellate 1 pattern of electromagnetic shielding material and line at interval, calculate the area A and area B that Fig. 4 represents after, its substitution following formula is calculated.
Aperture opening ratio (%)=(area B/area A) * 100 (%)
7. line is thick
Fixed with the surface roughness instrumentation.
Embodiment 1
As transparent resin base material, (contain transparent porous bed thickness 120 μ m at PETG film transparency carrier with the transparent porous layer with pellumina (bed thickness 20 μ m), the PICTORICO corporate system, on the opposing face of transparent porous layer trade name " TPX "), with the thickness after the sclerosis is the mode of 2 μ m, with the UV cured type acrylate hard coating agent of Meyer rod coating (big Japanese coating society system, trade name " UVclear " solid component concentration 50 weight %), be 300mJ/cm with ultraviolet ray with the exposure 80 ℃ of dryings after 2 minutes
2Irradiation forms hard conating.
On the porous area of this film, by screen process press (NEWLONG SEIMITSUKOGYO corporate system), use conductive paste (Teng Cang changes into society's system, trade name " DOTITEXA-9080 "), carry out the silk screen printing of clathrate pattern.
On the 500 purpose stainless steel yarns of half tone use with the stainless steel wire braiding of diameter 18 μ m, be provided with the half tone (middle natural pond ART SCREEN corporate system) of the clathrate emulsion pattern of live width 20 μ m, decorative pattern spacing 250 μ m, aperture opening ratio 84.6%.
After the printing, with the silver compound of each film stick with paste electricity consumption heating hot blast 55 ℃ carry out calcining in 15 minutes after, carry out calcining in 30 minutes at 150 ℃, form the conductive part of describing clathrate square decorative pattern, make electromagnetic shielding material.
With the graticule of the conductive part of the electromagnetic shielding material that obtains with light microscope (multiplying power: * 100) observe, almost not broken string and line ooze out (line chap) (Fig. 1).
Comparative example 1
As transparent resin base material, use PETG film (Japan weaving society system of the thick 175 μ m that transparent porous layer is not set, trade name " A4100 "), on its easy adhesive surface, with the thickness after the sclerosis is the mode of 2 μ m, with the UV cured type acrylate hard coating agent of Meyer rod coating (big Japanese coating society system, trade name " UVclear " solid component concentration 50 weight %), 80 ℃ of dryings after 2 minutes with ultraviolet be 300mJ/cm with the exposure
2Irradiation forms hard conating, and in addition, other make electromagnetic shielding material similarly to Example 1.On the opposing face of the hard conating that does not have this film, carry out silk screen printing.
With the graticule of the conductive part of the electromagnetic shielding material that obtains with light microscope (multiplying power: * 100) observe, find to take place ooze out (Fig. 2) of a lot of oligomer and line.
Comparative example 2
Substitute the silver compound contain emboliform silver oxide and uncle's aliphatic acid silver, solvent and stick with paste (Teng Cang changes into society's system), (the made SW-1100-1 composition of ASAHI chemical research compares: silver particles (particle diameter 3～5 μ m) 58.0～64.0% to use the silver of polymer type to stick with paste, carbon dust (primary particle 0.1 μ m or littler) 0.8～1.2%, mylar 11.0～14.0%, additive 0.05～0.15%, ethyl carbitol acetic acid esters (residual amount) viscosity 200～300ps (VISCOTESTER VT-04 type)), in addition, make electromagnetic shielding material similarly to Example 1.With the graticule of the conductive part of the electromagnetic shielding material that obtains with light microscope (multiplying power: * 100) observe, find to take place ooze out (Fig. 3) of a lot of broken strings and line.
The electromagnetic shielding effect of the electromagnetic shielding material of the foregoing description 1, comparative example 1,2, full light transmittance, turbidity value, the evaluation result of sheet resistor etc. is illustrated in the table 1.
[table 1]
| Electromagnetic shielding effect (d B) | Full light transmittance (%) | Turbidity value | Sheet resistor (Ω/) | Live width (μ m) | Aperture opening ratio (%) | Line thick (μ m) | |||
| 100MHz | 300MHz | 500MHz | |||||||
| Embodiment 1 | 31 | 33 | 39 | 73.8 | 5.6 | 0.645 | 22.0 | 83.2 | 2.5 |
| Comparative example 1 | 35 | 32 | 36 | 54.0 | 5.1 | 0.526 | 58.0 | 59.0 | 1.8 |
| Comparative example 2 | 39 | 33 | 33 | 66.5 | 10.3 | 1.672 | 45.9 | 66.7 | 2.0 |
Claims (14)
1. the manufacture method of an electromagnetic shielding material, it is characterized in that, contain at least a kind of this transparent porous aspect that is selected from oxide ceramics, non-oxide ceramics and the metal possessing as the transparent resin base material of the transparent porous layer of principal component, the conductive paste that will contain particle shape silver oxide, uncle's aliphatic acid silver and solvent carries out after the silk screen printing with the geometry pattern, with the transparent resin base material heat treated of this printing, on this transparent porous aspect, form the conductive part of geometry pattern.
2. the manufacture method of putting down in writing according to claim 1 is characterized in that, described transparent resin base material has hard conating on the face opposite with transparent porous layer.
3. according to claim 1 or 2 manufacture methods of being put down in writing, it is characterized in that it directly is that 2 μ m or lower particle shape silver oxide, total carbon atom number are the silver salt of uncle's aliphatic acid of 5～30 and will be selected from the ether-ether class of aromatic hydrocarbon, ethylene glycol, the ether-ether class of propylene glycol and at least a kind of solvent as principal component in the terpineol that described conductive paste contains averaged particles.
4. according to claim 1 or 2 manufacture methods of being put down in writing, it is characterized in that described transparent porous layer thickness is about 0.05～20 μ m.
5. according to claim 1 or 2 manufacture methods of being put down in writing, it is characterized in that, described transparent porous layer contains at least a kind of atomic aggregate as principal component that will be selected from silica, titanium oxide and the aluminium oxide, and has pore between this particulate.
6. the manufacture method of putting down in writing according to claim 5 is characterized in that, described atomic averaged particles directly is about 10～100nm, and described fine pore is about 10～100nm.
7. the manufacture method of putting down in writing according to claim 1, it is characterized in that described transparent porous layer is to form by being selected from a kind of method that intaglio plate coating, hectograph coating, comma coating, mouthful mould coating, slit coating, spray-painting, plating be coated with in method, sol-gel process, LB embrane method, CVD, evaporation, sputter, the ion plating.
8. according to the manufacture method of claim 1 or 2 electromagnetic shielding materials of being put down in writing, it is characterized in that the temperature of described heat treated is about 150～200 ℃.
9. according to claim 1 or 2 manufacture methods of being put down in writing, it is characterized in that the resin of described transparent resin base material is at least a kind that is selected from mylar, polycarbonate resin, poly-(methyl) acrylate, silicone resin, cyclic polyolefin resin, polyarylate resin and the polyethersulfone resin.
10. according to claim 1 or 2 manufacture methods of being put down in writing, it is characterized in that described transparent resin base material is sheet, membranaceous or tabular.
11. an electromagnetic shielding material is characterized in that, it is to make by the manufacture method that claim 1 or 2 is put down in writing, and the live width of the geometry pattern of conductive part is about 10～30 μ m, and aperture opening ratio is about 80～95%.
12. membranaceous electromagnetic shielding material, it is to be selected from oxide ceramics possessing to contain, on at least a kind of this transparent porous aspect in non-oxide ceramics and the metal as the transparent resin base material of the transparent porous layer of principal component, electromagnetic shielding material with conductive part of geometry pattern, the conductive part of described geometry pattern is to contain particle shape silver oxide, the conductive paste of uncle's aliphatic acid silver and solvent carries out after the silk screen printing with the geometry pattern, transparent resin base material heat treated with this printing, on this transparent porous aspect, form, wherein, the full light transmittance of described electromagnetic shielding material is 72～91%, turbidity value is 0.5～6%, sheet resistance value is 5 Ω/ or littler, the live width of the geometry pattern of described conductive part is about 10～30 μ m, and aperture opening ratio is about 80～95%.
13. the electromagnetic shielding filter that plasma display panel (PDP) is used is characterized in that, contains claim 11 or 12 electromagnetic shielding materials of being put down in writing.
14. on transparent porous aspect, form the method for the conductive part of geometry pattern, it is characterized in that, contain at least a kind of this transparent porous aspect that is selected from oxide ceramics, non-oxide ceramics and the metal possessing as the transparent resin base material of the transparent porous layer of principal component, the conductive paste that will contain particle shape silver oxide, uncle's aliphatic acid silver and solvent with the geometry pattern carries out after the silk screen printing, with the transparent resin base material heat treated of this printing.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP153343/2004 | 2004-05-24 | ||
| JP2004153343 | 2004-05-24 | ||
| PCT/JP2005/009173 WO2005115070A1 (en) | 2004-05-24 | 2005-05-19 | Electromagnetic wave shielding material and process for producing the same |
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| Publication Number | Publication Date |
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| CN1957650A CN1957650A (en) | 2007-05-02 |
| CN1957650B true CN1957650B (en) | 2010-06-16 |
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| CN200580016522XA Expired - Fee Related CN1957650B (en) | 2004-05-24 | 2005-05-19 | Electromagnetic wave shielding material and process for producing the same |
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| Country | Link |
|---|---|
| US (1) | US8168252B2 (en) |
| EP (1) | EP1758443B1 (en) |
| JP (1) | JP4538690B2 (en) |
| KR (1) | KR100868294B1 (en) |
| CN (1) | CN1957650B (en) |
| WO (1) | WO2005115070A1 (en) |
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| JP4679087B2 (en) * | 2004-07-09 | 2011-04-27 | グンゼ株式会社 | Transparent sheet heating element and manufacturing method thereof |
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| WO2007088896A1 (en) * | 2006-01-31 | 2007-08-09 | Fujifilm Corporation | Method for producing conductive film, light-transmitting electromagnetic shielding film, optical filter and plasma display panel |
| JP2008042021A (en) * | 2006-08-08 | 2008-02-21 | Bridgestone Corp | Light-transmitting electromagnetic wave shielding window material, and method and apparatus for producing the same |
| JP2008250244A (en) * | 2007-03-30 | 2008-10-16 | Gunze Ltd | Multilayer optical film |
| JP2008276220A (en) * | 2007-04-27 | 2008-11-13 | Samsung Sdi Co Ltd | Filter and plasma display device |
| EP2009977A3 (en) | 2007-05-09 | 2011-04-27 | FUJIFILM Corporation | Electromagnetic shielding film and optical filter |
| JP2009084400A (en) * | 2007-09-28 | 2009-04-23 | Gunze Ltd | Near-infrared absorbing pressure-sensitive adhesive composition and multilayer optical film |
| JP2009084399A (en) * | 2007-09-28 | 2009-04-23 | Gunze Ltd | Near-infrared absorbing pressure-sensitive adhesive composition and multilayer optical film |
| CN102067245A (en) | 2008-07-04 | 2011-05-18 | 户田工业株式会社 | Transparent electrically conductive transfer plate and production method therefor, transparent electrically conductive base, method for producing transparent electrically conductive base using transparent electrically conductive transfer plate, and molded product using the transparent conductive substrate |
| DE102010044326A1 (en) * | 2010-09-03 | 2012-03-08 | Heraeus Materials Technology Gmbh & Co. Kg | Use of aliphatic hydrocarbons and paraffins as solvents in silver pastes |
| CN102553814B (en) * | 2010-12-31 | 2014-03-12 | 中国科学院金属研究所 | Wave-absorbing functional protecting coating on surface of aluminum alloy and preparation method thereof |
| JP4933674B1 (en) * | 2011-08-20 | 2012-05-16 | 仁 新井 | Copper paste for electrodes. |
| JP5584737B2 (en) * | 2012-07-10 | 2014-09-03 | 旭化成せんい株式会社 | Noise suppression cable |
| CN102766370B (en) * | 2012-07-17 | 2014-09-17 | 西安亨孚新材料科技有限公司 | Organosilicon special coating |
| RU2545562C2 (en) * | 2013-07-26 | 2015-04-10 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский Государственный политехнический университет" | Method of forming radar-absorbent topologies on carriers |
| US20160330835A1 (en) * | 2014-01-24 | 2016-11-10 | Toppan Forms Co., Ltd. | Wiring board |
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| JP6347373B2 (en) * | 2017-02-17 | 2018-06-27 | 尾池工業株式会社 | Transparent conductive substrate and laminate for producing the same |
| WO2018163584A1 (en) * | 2017-03-10 | 2018-09-13 | マクセルホールディングス株式会社 | Electromagnetic wave absorbing sheet |
| CN110740626B (en) * | 2018-10-29 | 2020-11-03 | 嘉兴学院 | Preparation method of composite electromagnetic shielding material of copper and ceramic powder |
| CN111511181B (en) * | 2020-05-18 | 2022-08-12 | 深圳先进技术研究院 | Patterned electromagnetic shielding material and preparation method and application thereof |
| CN115232425B (en) * | 2022-08-09 | 2024-01-30 | 广东思泉新材料股份有限公司 | Low-dielectric high-heat-conductivity shielding dispersion, preparation method thereof and prepared shielding film |
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- 2005-05-19 JP JP2006513721A patent/JP4538690B2/en not_active Expired - Fee Related
- 2005-05-19 WO PCT/JP2005/009173 patent/WO2005115070A1/en active Application Filing
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| Publication number | Publication date |
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| US8168252B2 (en) | 2012-05-01 |
| EP1758443A4 (en) | 2009-05-06 |
| EP1758443A8 (en) | 2007-06-13 |
| US20070212536A1 (en) | 2007-09-13 |
| JPWO2005115070A1 (en) | 2008-03-27 |
| EP1758443A1 (en) | 2007-02-28 |
| CN1957650A (en) | 2007-05-02 |
| KR100868294B1 (en) | 2008-11-11 |
| EP1758443B1 (en) | 2012-08-15 |
| WO2005115070A1 (en) | 2005-12-01 |
| KR20070020045A (en) | 2007-02-16 |
| JP4538690B2 (en) | 2010-09-08 |
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